CN112323024A - High-strength antioxidant coating and preparation method and application thereof - Google Patents
High-strength antioxidant coating and preparation method and application thereof Download PDFInfo
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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- C23C14/0021—Reactive sputtering or evaporation
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/106—Coating with metal alloys or metal elements only
Abstract
The invention belongs to the technical field of metal surface coatings, and particularly relates to a high-strength antioxidant coating and a preparation method and application thereof. The high-strength oxidation resistant coating provided by the invention has an AlCoCrFeNi layer and Cr2A multi-layer structure with periodically arranged AlC layers, and AlCoCrFeNi layer and Cr layer2The thickness ratio of the AlC layer is (1-3): 1, wherein the AlCoCrFeNi layer ensures a coatingHigh oxidation resistance of, said Cr2The AlC layer is favorable for reducing the stress of the coating and enhancing the strength of the coating, and the AlCoCrFeNi layer and the Cr layer2The AlC layers are alternately and circularly stacked, and the structural characteristic can block the penetrating growth of columnar crystals, prevent penetrating defects and further improve the oxidation resistance of the coating.
Description
Technical Field
The invention belongs to the technical field of metal surface coatings, and particularly relates to a high-strength antioxidant coating and a preparation method and application thereof.
Background
In recent years, with the continuous improvement of energy levels of materials to be processed (high precision, high efficiency and high speed), the emergence of new materials which are difficult to cut and have high strength, high toughness and the like (such as titanium alloy, high-silicon aluminum alloy, carbon fiber composite material, dual-phase steel and the like for aerospace, automobiles, ocean engineering equipment and the like), the development of dry type, green type and other special processing requirements (oil-free and environment-friendly) is provided, higher challenges are provided for the development of metal coatings, and the traditional hard coating with low hardness and poor oxidation resistance is difficult to meet the rigorous application requirements.
Disclosure of Invention
In view of the above, the invention provides a high-strength oxidation-resistant coating, and a preparation method and an application thereof.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a high-strength oxidation-resistant coating, which comprises a transition layer and a composite layer deposited on the surface of the transition layer;
the composite layer comprises AlCoCrFeNi layers and Cr layers which are alternately and circularly laminated2An AlC layer;
the AlCoCrFeNi layer and the Cr layer2The single-layer thickness ratio of the AlC layer is (1-3): 1.
preferably, the transition layer comprises a metal bottom layer and an intermediate layer deposited on the surface of the metal bottom layer;
the metal bottom layer comprises an Al layer or a Cr layer;
when the metal underlayer comprises an Al layer, the intermediate layer comprises an AlN layer;
when the metal underlayer comprises a Cr layer, the intermediate layer comprises a CrN layer.
Preferably, the thickness ratio of the metal bottom layer to the intermediate layer is 1: (1-3); the thickness of the metal bottom layer is 20-300 nm.
Preferably, the single-layer thickness of the AlCoCrFeNi layer is 0.2-0.6 mu m, the number of the AlCoCrFeNi layers is 4-10, and the Cr layer is2The number of AlC layers is 3-10.
The invention provides a preparation method of a high-strength antioxidant coating, which comprises the following steps:
depositing a transition layer on the surface of the substrate;
alternately and circularly depositing AlCoCrFeNi layers and Cr on the surface of the transition layer2An AlC layer, forming a composite layer on the surface of the transition layer to obtain a coating pre-sample, wherein the AlCoCrFeNi layer and the Cr layer2The single-layer deposition thickness ratio of the AlC layer is (1-3): 1;
and annealing the coating pre-sample to obtain the high-strength oxidation-resistant coating.
Preferably, the depositing the transition layer comprises:
taking an Al target or a Cr target as a target material, and performing first arc ion plating on the surface of the substrate in an argon atmosphere to form a metal bottom layer, wherein the conditions of the first arc ion plating comprise: the arc current is 50-100A, the substrate bias voltage is-60 to-200V, and the pressure of the argon is 0.6-2.0 Pa;
using Al target or Cr target as target material in N2And argon gas, and performing second arc ion plating on the surface of the metal bottom layer to form an intermediate layer, wherein the conditions of the second arc ion plating comprise: the arc current is 50-100A, the substrate bias voltage is-60-200V, the pressure of argon in the mixed atmosphere is 0.6-2.0 Pa, and N is2The pressure of the pressure is 3-6 Pa;
the target material for depositing the middle layer is the same as the target material for depositing the metal bottom layer.
Preferably, the AlCoCrFeNi layer and the Cr are deposited in an alternating cycle2The AlC layer includes: alternately taking an AlCoCrFeNi high-entropy alloy target and a CrAl alloy target as target materials,arc ion plating is alternately carried out on the surface of the transition layer, and AlCoCrFeNi layers and Cr are alternately and circularly formed2An AlC layer;
the conditions for depositing the AlCoCrFeNi layer comprise the following steps: the arc current is 80-120A, the substrate bias voltage is-80-200V, the deposition atmosphere is argon, and the pressure of the argon is 0.8-2.0 Pa;
depositing the Cr2The conditions of the AlC layer include: the arc current is 100-120A, the substrate bias voltage is-80-150V, the deposition atmosphere is a mixed gas of argon and hydrocarbon reaction gas, and the pressure of the mixed gas is 0.8-1.5 Pa; the hydrocarbon reaction gas is methane and/or acetylene.
Preferably, the preparation method of the AlCoCrFeNi high-entropy alloy target comprises the following steps:
al powder, Co powder, Cr powder, Fe powder and Ni powder are mixed according to a mol ratio of 1: 1: 1: 1: 1, mixing to obtain cladding powder;
cladding the cladding powder on the surface of a target substrate by using a plasma transfer arc welding technology to obtain an AlCoCrFeNi high-entropy alloy cladding layer;
and processing the target material substrate and the AlCoCrFeNi high-entropy alloy cladding layer into the AlCoCrFeNi high-entropy alloy target by utilizing a numerical control machine.
Preferably, the temperature of the annealing treatment is 300-700 ℃, and the time is 10-1000 h.
The invention also provides the application of the high-strength oxidation-resistant coating in the technical scheme or the high-strength oxidation-resistant coating obtained by the preparation method in the technical scheme in a metal surface coating.
Compared with the prior art, the invention has the following technical effects:
the high-strength oxidation-resistant coating provided by the invention comprises a transition layer and a composite layer deposited on the surface of the transition layer; the composite layer comprises AlCoCrFeNi layers and Cr layers which are alternately and circularly laminated2An AlC layer; the AlCoCrFeNi layer and the Cr layer2The single-layer thickness ratio of the AlC layer is (1-3): 1. the high-strength oxidation resistant coating provided by the invention has an AlCoCrFeNi layer and Cr2A multi-layer structure with periodically arranged AlC layers, and AlCoCrFeNi layer and Cr layer2Single layer of AlC layerThe thickness ratio is (1-3): 1, wherein the AlCoCrFeNi layer ensures high oxidation resistance of the coating, the Cr layer2The AlC layer is favorable for reducing the stress of the coating and enhancing the strength of the coating, and the AlCoCrFeNi layer and the Cr layer2The AlC layers are alternately and circularly stacked, and the structural characteristic can block the penetrating growth of columnar crystals, prevent penetrating defects and further improve the oxidation resistance of the coating. Moreover, the AlCoCrFeNi layer belongs to eutectic high-entropy alloy, has good ductility, and has better wettability and compatibility of the interface between the high-strength oxidation-resistant coating layers compared with the existing hard and soft multi-layer composite. The results of the examples show that the high-strength oxidation-resistant coating provided by the invention is excellent in the aspects of high hardness and oxidation resistance.
Drawings
FIG. 1 is a flow chart of the preparation of the high strength oxidation resistant coating prepared in example 1;
figure 2 is a schematic cross-sectional view of the high strength oxidation resistant coating prepared in example 1,
wherein, 1-metal bottom layer, 2-middle layer, 3-composite layer, 4-AlCoCrFeNi layer, 5-Cr2AlC layer, 6-base;
FIG. 3 is a schematic diagram showing the morphology and composition of the AlCoCrFeNi high-entropy alloy layer target material prepared in example 1;
FIG. 4 is the surface topography of the oxide layer of the high strength oxidation resistant coating prepared in example 1 at different times;
FIG. 5 shows the high strength oxidation resistant coating prepared in example 1 and Cr in comparative example 12A curve graph of AlC coating hardness along with pressing depth;
FIG. 6 shows the bonding strength (45N) between the high-strength oxidation-resistant coating prepared in example 1 and the substrate;
FIG. 7 shows Cr in comparative example 12The bonding force of the AlC coating and the substrate (the bonding force is 30N);
fig. 8 is a graph of the oxidation weight gain at 1000 c for the high strength oxidation resistant coating prepared in example 1 and the AlCoCrFeNi coating of comparative example 2.
Detailed Description
The invention provides a high-strength oxidation-resistant coating, which comprises a transition layer and a composite layer deposited on the surface of the transition layer;
the composite layer comprises AlCoCrFeNi layers and Cr layers which are alternately and circularly laminated2An AlC layer;
the AlCoCrFeNi layer and the Cr layer2The single-layer thickness ratio of the AlC layer is (1-3): 1.
in the present invention, the transition layer preferably includes a metal underlayer and an intermediate layer deposited on the surface of the metal underlayer; in the present invention, the metal underlayer preferably includes an Al layer or a Cr layer, and when the metal underlayer preferably includes an Al layer, the intermediate layer preferably includes an AlN layer; while the metal underlayer preferably comprises a Cr layer, the intermediate layer preferably comprises a CrN layer.
In the present invention, the thickness ratio of the metal underlayer and the intermediate layer is preferably 1: (1-3), more preferably 1: (1.5-2); the thickness of the metal bottom layer is preferably 20-300 nm, and more preferably 100-200 nm.
In the present invention, the composite layer includes AlCoCrFeNi layers and Cr layers alternately and cyclically stacked2An AlC layer; the invention is used for preparing the AlCoCrFeNi layer and the Cr2The sequence of AlC layers alternately and circularly stacked has no special requirement, and in the invention, the surface of the transition layer can be an AlCoCrFeNi layer or a Cr layer2And the surface of the transition layer is an AlCoCrFeNi layer in the specific embodiment of the invention. The invention has no special requirement on the arrangement of the outermost layer of the composite layer, and in the specific embodiment of the invention, the outermost layer of the composite layer is an AlCoCrFeNi layer. In the invention, the AlCoCrFeNi layer and the Cr layer2At least one AlC layer is arranged. In a specific embodiment of the invention, the surface of the transition layer is an AlCoCrFeNi layer in order to make the composite layer and the transition layer better combined; the outermost layer of the composite layer is an AlCoCrFeNi layer so as to enable the oxidation resistance of the composite layer to be stronger.
In the invention, the AlCoCrFeNi layer and the Cr layer2The single-layer thickness ratio of the AlC layer is (1-3): 1, preferably (1.5-2): 1.
in the invention, the thickness of the single layer of the AlCoCrFeNi layer is preferably 0.2-0.6 mu m, more preferably 0.35-0.5 mu m, and the number of the layers of the AlCoCrFeNi layer is preferably 4-10A layer, more preferably 5 to 8 layers, of Cr2The number of the AlC layers is preferably 3-10, and more preferably 4-8; preferred AlCoCrFeNi layer ratio Cr2The number of AlC layers is one layer more. In a specific embodiment of the invention, the number of the AlCoCrFeNi layers is 4, and the Cr layers are2When the number of the AlC layers is 3, the composite layer specifically comprises: AlCoCrFeNi layer-Cr2AlC layer-AlCoCrFeNi layer-Cr2AlC layer-AlCoCrFeNi layer-Cr2AlC layer-AlCoCrFeNi layer.
The high-strength oxidation resistant coating provided by the invention has an AlCoCrFeNi layer and Cr2AlC layer of multilayer structure, and AlCoCrFeNi layer and Cr layer2The single-layer thickness ratio of the AlC layer is (1-3): 1, wherein the AlCoCrFeNi layer ensures high oxidation resistance of the coating, the Cr layer2The AlC layer is favorable for reducing the stress of the coating and enhancing the strength of the coating, and the AlCoCrFeNi layer and the Cr layer2The AlC layers are alternately and circularly stacked, and the structural characteristic can block the penetrating growth of columnar crystals, prevent penetrating defects and further improve the oxidation resistance of the coating.
The invention provides a preparation method of a high-strength antioxidant coating, which comprises the following steps:
depositing a transition layer on the surface of the substrate;
alternately and circularly depositing AlCoCrFeNi layers and Cr on the surface of the transition layer2An AlC layer, forming a composite layer on the surface of the transition layer to obtain a coating pre-sample, wherein the AlCoCrFeNi layer and the Cr layer2The single-layer deposition thickness ratio of the AlC layer is (1-3): 1;
and annealing the coating pre-sample to obtain the high-strength oxidation-resistant coating.
The invention deposits a transition layer on the surface of a substrate to obtain the transition layer.
The substrate is a device needing antioxidant protection, and in a specific embodiment of the invention, the substrate is preferably die steel or cutter steel.
According to the invention, before the transition layer is deposited on the surface of the substrate, the substrate is preferably pretreated, in the invention, the pretreatment preferably comprises cleaning, drying and etching which are sequentially carried out, in the invention, the cleaning preferably comprises degreasing agent cleaning, alcohol cleaning and acetone cleaning which are sequentially carried out, and the invention has no special requirements on the specific implementation modes of the cleaning and the drying and can adopt a mode which is well known to a person skilled in the art.
In the invention, the etching mode is preferably ion etching, ions used by the ion etching are preferably argon ions, the argon ions are obtained by ionizing argon by an ion source, and the gas flow of the argon is preferably 20-70 sccm, more preferably 30-45 sccm; the current of the ion source is preferably 0.1-0.3A, more preferably 0.15-0.25A, and the ion source is preferably a linear anode ion source; the etching time is preferably 10-50 min, more preferably 25-35 min, and the etching pressure is preferably 0.2-0.6 Pa, more preferably 0.3-0.5 Pa. The present invention does not require any particular implementation of the ion etching, and can be implemented in a manner known to those skilled in the art. In the embodiment of the present invention, the specific process of the ion etching is as follows: and (3) putting the cleaned and dried substrate into a vacuum coating chamber, introducing argon into the vacuum cavity through an anode ion source, and etching the substrate by utilizing ionized argon ions. The etching time is 30min and the pressure is 0.5 Pa.
In the present invention, the depositing the transition layer preferably includes: taking an Al target or a Cr target as a target material, and performing first arc ion plating on the surface of the substrate in an argon atmosphere to form a metal bottom layer, wherein the conditions of the first arc ion plating preferably comprise: the arc current is preferably 50-100A, more preferably 65-75A; the substrate bias is preferably-60 to-200V, more preferably-95 to-120V, and most preferably-100 to-110V; the pressure intensity of the argon is preferably 0.6-2.0 Pa; more preferably 0.8 to 1.5Pa, and most preferably 1.0 to 1.2 Pa. In the invention, the deposition thickness of the metal bottom layer is preferably 20-300 nm, more preferably 200-250 nm, and the deposition time is preferably 15-30 min, more preferably 18.5-25 min. In the present invention, there is no particular requirement for the specific implementation of the arc ion plating method, and the implementation may be performed by a method known to those skilled in the art.
After forming the metal underlayer, the present invention preferably formsAl target or Cr target as target material in the presence of N2And argon gas, and performing second arc ion plating on the surface of the metal bottom layer to form an intermediate layer, wherein the conditions of the second arc ion plating preferably comprise: the arc current is preferably 50-100A, more preferably 60-80A; the substrate bias is-60 to-200V, more preferably-95 to-150V, and most preferably-100 to-120V; the pressure of argon in the mixed atmosphere is preferably 0.6-2.0 Pa, more preferably 0.8-1.5 Pa, and most preferably 1.0-1.2 Pa, and the N2The pressure of (A) is 3 to 6Pa, more preferably 3.5 to 5.5Pa, and most preferably 4 to 5 Pa. In the invention, the target material for depositing the middle layer is the same as the target material for depositing the metal bottom layer.
In the present invention, the ratio of the deposition thickness of the metal underlayer to the deposition thickness of the intermediate layer is preferably 1: (1-3), more preferably 1: (2-2.5).
In the invention, the deposition time of the intermediate layer is preferably 25-45 min, and more preferably 30-40 min.
After the transition layer is obtained, the AlCoCrFeNi layer and the Cr layer are alternately and circularly deposited on the surface of the transition layer2And an AlC layer, forming a composite layer on the surface of the transition layer to obtain a coating pre-sample.
In the invention, the AlCoCrFeNi layer and the Cr are deposited alternately and circularly2The AlC layer preferably includes: alternately taking AlCoCrFeNi high-entropy alloy targets and CrAl alloy targets as target materials, alternately performing arc ion plating on the surface of the transition layer, and alternately and circularly forming AlCoCrFeNi layers and Cr layers2An AlC layer; the AlCoCrFeNi layer and the Cr layer2The single-layer deposition thickness ratio of the AlC layer is (1-3): 1, preferably (1.5-2): 1. in the invention, the deposition thickness of the AlCoCrFeNi monolayer is preferably 0.2-0.6 mu m, more preferably 0.35-0.5 mu m, the number of deposition layers of the AlCoCrFeNi layer is preferably 4-10, more preferably 5-8, and the Cr layer is preferably an inner layer2The preferred number of the deposited AlC layers is 3-10, and the more preferred number is 4-8. In the invention, the deposition time of the composite layer is preferably 2-4 h, and more preferably 2.5-3 h. The invention is used for preparing the AlCoCrFeNi layer and the Cr2The deposition sequence of the AlC layer has no special requirements, and the two layers are ensured to be alternately and circularly deposited. In the present inventionIt is to be understood that the specific embodiment of the arc ion plating method is not particularly limited, and may be performed in a manner known to those skilled in the art.
In the invention, the target material for depositing the AlCoCrFeNi layer is preferably an AlCoCrFeNi high-entropy alloy target, and the arc current is preferably 80-120A, more preferably 100-115A; the substrate bias voltage is preferably-60 to-200V, more preferably-85 to-120V; the deposition atmosphere is preferably argon, the pressure of the argon is preferably 0.6-2.0 Pa, more preferably 1.0-1.2 Pa, and the single-layer deposition time of the AlCoCrFeNi layer is preferably 20-30 min.
In the invention, the preparation method of the AlCoCrFeNi high-entropy alloy target preferably comprises the following steps:
al powder, Co powder, Cr powder, Fe powder and Ni powder are mixed according to a mol ratio of 1: 1: 1: 1: 1, mixing to obtain cladding powder;
cladding the cladding powder on the surface of a target substrate by using a plasma transfer arc welding technology to obtain an AlCoCrFeNi high-entropy alloy cladding layer;
and processing the target substrate and the AlCoCrFeNi high-entropy alloy cladding layer into the AlCoCrFeNi high-entropy alloy target by utilizing a numerical control machine.
The invention relates to a method for preparing a high-performance composite material by mixing Al powder, Co powder, Cr powder, Fe powder and Ni powder according to a mol ratio of 1: 1: 1: 1: 1, mixing to obtain cladding powder.
In the invention, the purities of the Al powder, the Co powder, the Cr powder, the Fe powder and the Ni powder are preferably more than or equal to 99.9% independently, in the invention, the mixing mode is preferably mechanical grinding, and the invention has no special requirement on the operation of a matrix of the mechanical grinding and can realize uniform mixing. The invention has no special requirements on the sources of the Al powder, the Co powder, the Cr powder, the Fe powder and the Ni powder, and can be prepared by adopting spherical powder with 100-200 meshes.
After the cladding powder is obtained, the cladding powder is cladded on the surface of a target material substrate by using a plasma transfer arc welding technology to obtain the AlCoCrFeNi high-entropy alloy cladding layer.
In the invention, the arc current for cladding by using the plasma transferred arc welding technology is preferably 90-120A, and more preferably 100-115A; the cladding walking speed is preferably 6 mm/min; the powder feeding amount is preferably 35%; the ion gas flow is preferably 1.0-2.0L/min, more preferably 1.5L/min, and the protective gas flow is preferably 10-30L/min, more preferably 15L/min; the preferable flow rate of the powder conveying gas is 2.5L/min; the amplitude width is preferably 20 mm; the overlapping rate is preferably 20%, and in the present invention, the cladding method using the plasma transferred arc welding technique is preferably a multi-pass multi-layer cladding method. The present invention does not require special implementation of the plasma transferred arc welding technique, and can be implemented in a manner well known to those skilled in the art. In the invention, the thickness of the cladding substrate is preferably 15-30 mm, more preferably 20-25 mm, and the thickness of the AlCoCrFeNi high-entropy alloy cladding layer is preferably 10-20 mm.
The invention has no special requirements on the type and source of the cladding substrate, in the embodiment of the invention, the cladding substrate is an Al alloy plate, and the thickness of the Al alloy plate is preferably 15-30 mm, and more preferably 20-25 mm.
In the invention, the length of the AlCoCrFeNi high-entropy alloy cladding layer is preferably 80-100 mm; the width is preferably 80-100 mm; the thickness is preferably 5 to 10 mm.
After the AlCoCrFeNi high-entropy alloy cladding layer is obtained, the cladding substrate and the AlCoCrFeNi high-entropy alloy cladding layer are processed into the AlCoCrFeNi high-entropy alloy target by utilizing a numerical control machine.
The present invention does not require any particular method for said processing, and methods known to those skilled in the art may be used.
In the present invention, the Cr is deposited2The target material of the AlC layer is preferably CrAl alloy target, the arc current is preferably 100-120A, and more preferably 110-115A; the substrate bias voltage is preferably-80 to-150V, more preferably-85 to-135V, and most preferably-90 to-110V; the deposition atmosphere is preferably a mixed gas of argon and a hydrocarbon reaction gas, the hydrocarbon reaction gas is preferably methane and/or acetylene, and is more preferably methane or acetylene; the gas flow ratio of the hydrocarbon reaction gas to the mixed gas is preferably 5-15%, and more preferably 7.5-12%; in the present invention, the pressure of the mixed gas of argon and hydrocarbon reaction gas is preferably 0.8About 1.5Pa, more preferably about 1.0 to about 1.2Pa, and in the present invention, the Cr is2The single-layer deposition time of the AlC layer is preferably 20-30 min. The invention has no special requirements on the source of the CrAl composite target and can adopt a product sold in the market.
After the coating pre-sample is obtained, annealing treatment is carried out on the coating pre-sample to obtain the high-strength oxidation-resistant coating.
In the invention, the annealing treatment temperature is preferably 300-700 ℃, more preferably 350-650 ℃, and most preferably 400-600 ℃; the time is preferably 10 to 1000 hours, more preferably 50 to 800 hours, and most preferably 100 to 600 hours. In the present invention, the annealing treatment is preferably performed under vacuum or a protective atmosphere, which is preferably argon; when the annealing treatment is performed under vacuum, the degree of vacuum is preferably 1.0 × 10-3～3.0×10-2Pa, more preferably 5.0X 10-3～25×10-3Pa, most preferably 10X 10-3～15×10-3Pa; when the annealing treatment is performed under a protective atmosphere, the pressure of the protective atmosphere is preferably 101.325 × 103Pa。
In the present invention, Cr is increased by an annealing process2The crystallinity of the AlC layer reduces the stress between films, and realizes the shaping of the composite coating.
The invention also provides the application of the high-strength oxidation-resistant coating in the technical scheme or the high-strength oxidation-resistant coating obtained by the preparation method in the technical scheme in a metal surface coating.
In the invention, the surface of the cemented carbide hobbing cutter should preferably be applied, and in the invention, the specific method for applying is as follows: and depositing a high-strength oxidation resistant coating on the surface of the hard alloy hobbing cutter.
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
Al powder, Co powder, Cr powder, Fe powder and Ni powder with the purity of 99.9 percent are mixed according to the mol ratio of 1: 1: 1: 1: 1, mechanically grinding the mixture uniformly to obtain cladding powder; by utilizing a plasma transferred arc technology, arc current is 100A, ionic gas flow is 1.5L/min, cladding traveling speed is 6mm/min, powder feeding amount is 35%, protective gas flow is 15L/min, powder feeding gas flow is 2.5L/min, amplitude width is 20mm, lap ratio is 20%, multiple-pass multilayer cladding is carried out, an AlCoCrFeNi high-entropy alloy cladding layer is cladded on the surface of an Al alloy plate with the thickness of 20mm, the size length of the cladding layer is 100mm, the width is 100mm, and the thickness is 15 mm; then processing the substrate and the AlCoCrFeNi high-entropy alloy cladding layer into an AlCoCrFeNi high-entropy alloy target;
according to the preparation flow shown in fig. 1, the cleaned and dried substrate is placed into a vacuum cavity, argon gas is introduced into the vacuum cavity at 45sccm, the current of a linear anode ion source is set to be 0.3A, the negative bias voltage of the substrate is set to be-180V, and the substrate is etched for 30min by utilizing ionized argon ions;
depositing a Cr bottom layer on the surface of the pretreated substrate by adopting an arc ion plating technology, wherein a target material is a Cr target, an arc current is 80A, a deposition gas is Ar gas, the pressure of the Ar gas is 1.2Pa, and the deposition thickness is 225 nm; then N is introduced2Depositing a CrN intermediate layer, wherein the pressure of Ar gas is 0.8Pa, and N2The gas pressure is 4Pa, the arc current is 80A, the bias voltage is-120V, and the deposition thickness is about 670 nm; obtaining a transition layer;
alternately and circularly laminating and depositing AlCoCrFeNi layers and Cr layers on the surface of the transition layer by adopting an arc ion plating technology2The target material for depositing the AlCoCrFeNi layer is an AlCoCrFeNi high-entropy alloy target, the arc current is 90A, the negative bias of the substrate is-120V, the deposition gas is Ar gas, the pressure of the Ar gas is 1.2Pa, and the deposition thickness is about 900 nm; the number of deposited layers is 4; deposition of Cr2The target material of the AlC layer is CrAl alloy target, the arc current is 70A, the negative bias of the substrate is-150V, and the deposition gas is Ar and CH4Mixed gas, CH4The gas flow rate of the mixed gas is 10%, the pressure of the mixed gas is 1.5Pa, and the deposition thickness is 600 nm; the number of deposited layers is 3; obtaining a coating pre-sample;
carrying out heat treatment on the coating pre-sample under the protection of argon, wherein the Ar gas pressure is 105Pa, the annealing temperature is 600 ℃, and the annealing time is 50h, so that the high-strength oxidation-resistant coating is obtained.
The cross-sectional view of the high-strength oxidation-resistant coating is shown in FIG. 2, and the topography is shown in FIG. 3.
Comparative example 1
Comparative example 1 and example 1 were prepared in the same manner except that: depositing Cr only on the surface of the transition layer by arc ion plating technology2An AlC layer was deposited to a thickness of about 5.25 μm.
Comparative example 2
Comparative example 1 and example 1 were prepared in the same manner except that: only an AlCoCrFeNi layer is deposited on the surface of the transition layer by adopting an arc ion plating technology, and the deposition thickness is 5.28 mu m.
Test example 1
An oxidation experiment is carried out on the high-strength oxidation-resistant coating prepared in the embodiment 1, the experimental method is that the product prepared in the embodiment 1 is placed in a muffle furnace to carry out air natural convection and heat preservation at 1050 ℃ for 5 hours and 50 hours, and the obtained surface morphology of an oxidation layer is shown in fig. 4, wherein (a) is the surface morphology of the oxidation layer after oxidation at 1050 ℃ for 5 hours, and (b) is the surface morphology of the oxidation layer after oxidation at 1050 ℃ for 50 hours, and the results can be obtained through (a) and (b) in fig. 4.
Test example 2
The products obtained in example 1 and comparative example 1 were subjected to a coating hardness test experiment, the experimental apparatus is a nanoindenter, and the curve of hardness variation with press-in depth is shown in fig. 5, which can be seen from fig. 5, and it can be seen that the high-strength oxidation-resistant coating prepared in example 1 of the present invention and the composite layer prepared in comparative example 1 have the same trend of coating hardness variation with the increase of press-in depth, but the hardness of the high-strength oxidation-resistant coating prepared in example 1 is greater than that of the composite layer in comparative example 1, which indicates that the high-strength oxidation-resistant coating prepared in example 1 has excellent strength.
Test example 3
The products obtained in example 1 and comparative example 1 were tested for their adhesion to the substrateExperiment, the experimental apparatus is a nano scratch apparatus, fig. 6 shows the bonding force between the high-strength oxidation-resistant coating prepared in example 1 and the substrate, the bonding force being 45N; FIG. 7 shows Cr in comparative example 12The bonding force between the AlC coating and the substrate is 30N; it is demonstrated that the high-strength oxidation-resistant coating prepared in example 1 has excellent bonding force.
Test example 4
The products obtained in example 1 and comparative example 2 were tested for coating oxidation weight gain at 1000 ℃ by placing the product in a crucible and weighing, then placing the crucible in a muffle furnace for natural convection at 1000 ℃ for heat preservation, taking out the crucible and the sample together every 25 hours and weighing, and recording the weight gain value each time. Fig. 8 is a graph of the oxidation weight gain of the high-strength oxidation-resistant coating prepared in example 1 and the composite layer in comparative example 2 at 1000 ℃, and it can be seen from fig. 8 that the weight gain of the high-strength oxidation-resistant coating prepared in example 1 is significantly lower than that of the product in comparative example 2 as the oxidation time increases, especially after the oxidation time is greater than 25 hours, which illustrates that the high-strength oxidation-resistant coating prepared in example 1 has excellent high-temperature oxidation resistance.
Test example 5
Depositing a high-strength antioxidant coating on the surface of a hard alloy hobbing cutter, and then cutting the undeposited hard alloy hobbing cutter and the hard alloy hobbing cutter deposited with the high-strength antioxidant coating on an NBP-1000 triaxial vertical machining center, wherein the machined gear material is 20CrMnTi (HRC 58-62), and the machining parameters are as follows: the processing speed is 750r/min, the feed per tooth is 0.28mm/r, the pressure angle is 20 degrees, and dry cutting is carried out.
20 hard alloy hobbing cutters which are not deposited are machined under the dry cutting condition, and 150 hobbing cutters which are deposited with the high-strength oxidation-resistant coatings can be machined, so that the service life of the hobbing cutters is prolonged by more than 7 times compared with the cutters which are not coated with the coatings.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. The high-strength oxidation-resistant coating is characterized by comprising a transition layer and a composite layer deposited on the surface of the transition layer;
the composite layer comprises AlCoCrFeNi layers and Cr layers which are alternately and circularly laminated2An AlC layer;
the AlCoCrFeNi layer and the Cr layer2The single-layer thickness ratio of the AlC layer is (1-3): 1.
2. the high strength oxidation resistant coating according to claim 1, wherein said transition layer comprises a metal underlayer and an intermediate layer deposited on the surface of the metal underlayer;
the metal bottom layer comprises an Al layer or a Cr layer;
when the metal underlayer comprises an Al layer, the intermediate layer comprises an AlN layer;
when the metal underlayer comprises a Cr layer, the intermediate layer comprises a CrN layer.
3. The high strength oxidation resistant coating of claim 2, wherein the ratio of the thickness of said metal underlayer to the thickness of said intermediate layer is 1: (1-3); the thickness of the metal bottom layer is 20-300 nm.
4. The high strength oxidation resistant coating of claim 1, wherein the AlCoCrFeNi layer has a single layer thickness of 0.2-0.6 μm, the number of AlCoCrFeNi layers is 4-10, and the Cr layer is2The number of AlC layers is 3-10.
5. The method for preparing a high-strength oxidation-resistant coating layer according to any one of claims 1 to 4, comprising the steps of:
depositing a transition layer on the surface of the substrate;
alternately and circularly depositing AlCoCrFeNi layers and Cr on the surface of the transition layer2An AlC layer, forming a composite layer on the surface of the transition layer to obtain a coating pre-sample, wherein the AlCoCrFeNi layer and the C layerr2The single-layer deposition thickness ratio of the AlC layer is (1-3): 1;
and annealing the coating pre-sample to obtain the high-strength oxidation-resistant coating.
6. The method of claim 5, wherein the depositing the transition layer comprises:
taking an Al target or a Cr target as a target material, and performing first arc ion plating on the surface of the substrate in an argon atmosphere to form a metal bottom layer, wherein the conditions of the first arc ion plating comprise: the arc current is 50-100A, the substrate bias voltage is-60 to-200V, and the pressure of the argon is 0.6-2.0 Pa;
using Al target or Cr target as target material in N2And argon gas, and performing second arc ion plating on the surface of the metal bottom layer to form an intermediate layer, wherein the conditions of the second arc ion plating comprise: the arc current is 50-100A, the substrate bias voltage is-60-200V, the pressure of argon in the mixed atmosphere is 0.6-2.0 Pa, and N is2The pressure of the pressure is 3-6 Pa;
the target material for depositing the middle layer is the same as the target material for depositing the metal bottom layer.
7. The method of claim 5, wherein the alternating cyclical deposition of AlCoCrFeNi layers and Cr2The AlC layer includes: alternately taking AlCoCrFeNi high-entropy alloy targets and CrAl alloy targets as target materials, alternately performing arc ion plating on the surface of the transition layer, and alternately and circularly forming AlCoCrFeNi layers and Cr layers2An AlC layer;
the conditions for depositing the AlCoCrFeNi layer comprise the following steps: the arc current is 80-120A, the substrate bias voltage is-80-200V, the deposition atmosphere is argon, and the pressure of the argon is 0.8-2.0 Pa;
depositing the Cr2The conditions of the AlC layer include: the arc current is 100-120A, the substrate bias voltage is-80-150V, the deposition atmosphere is a mixed gas of argon and hydrocarbon reaction gas, and the pressure of the mixed gas is 0.8-1.5 Pa; the hydrocarbon reaction gas is methane and/or acetylene.
8. The preparation method of claim 7, wherein the preparation method of the AlCoCrFeNi high-entropy alloy target comprises the following steps:
al powder, Co powder, Cr powder, Fe powder and Ni powder are mixed according to a mol ratio of 1: 1: 1: 1: 1, mixing to obtain cladding powder;
cladding the cladding powder on the surface of a target substrate by using a plasma transfer arc welding technology to obtain an AlCoCrFeNi high-entropy alloy cladding layer;
and processing the target material substrate and the AlCoCrFeNi high-entropy alloy cladding layer into the AlCoCrFeNi high-entropy alloy target by utilizing a numerical control machine.
9. The method according to claim 5, wherein the annealing is performed at a temperature of 300 to 700 ℃ for 10 to 1000 hours.
10. Use of the high-strength oxidation-resistant coating of any one of claims 1 to 4 or the high-strength oxidation-resistant coating obtained by the preparation method of any one of claims 5 to 9 in a metal surface coating.
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